Method of making sulfite liquor.



E.. K. MOORE Oz. R. E. WOLF. METHOD o? MAKING SU'LPITE LIQUOR.

APPLIUATION FILED DIEU. 31, l913.

Mmmm June 9, 19M

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HUGH K. MOORE AND ROBERT B. WDLlli, 0F BEHLXN, lillli] l'rlllllflPEllllltlsl.

lyceenne.

lpecflcation of Letters Patent.

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Application filed December 31, 1913. Serial lilo, 809,659.

To al( 'ic/rom. 'z may concern:

Be it known that we, lluou l. Mooier and lilonun'r ll. ll'onr, citizens ot the United States, and both residents of Berlin, in the county of Coos and State of New Hampshire, have invented certain new and useful Imi'irovements in Methods of Making Sullite Liquor, of which the following is a specifin cation.

lfhis invention has relation to the manufacture of sullite fiber in which the raw material is cooked in a digester in an acid liquor having therein more or less .tree or uncornhined sulfurous acid.

The object of the present invention is to provide an acid liquor havin a predetermined proportion of free suli'urous acid.

@n the accompanying drawings, We havey illustrated conventionally apparatus which embodies the invention and 'which may he utilized in carrying out our process.

rll`he figure illustrates a miner, a cooler for the gas, a sulfur burner, a refrigerator' tor the milk ot lime, a gas pump, and the various necessary connections.

it Will be understood that the mixing' apparatus7 which is illustrated upon the draivings, may loe substantially like that illustrated in United States Letters Patent No. 649,041, dated Mey 8, i900, but that the invention is not limited to the employment of that particulai` mixer, as any other form may he employed which is capable Jfor the purpose.

At l0 is illustrated crmventioluilly a por tion oi a sulfur burner for producing sulfur yilioiiidgas. ln the burner is burned either illl .sulfur or any ore coi'itaining` sulfur. From this burner, the products of combustion are conducted through a cooling' al'iparatus ll which condenses those gases having a volatilizing point higher than that ol the sulfur dioxid, before the remaining products ol combustion are delivered to the mixing' apparatus where they are mixed with the milk of linie or other solvent. Any suitable or usual form oi cooling` apparatus or condenser may be used lor this purpose. the tcmporature heine so regulated that the ,eases delivered from the cooler are al. a temperature of aj'iproximately 70 l1`. From this cooler7 the uncondensed gases may he forced llli or pumped hy a pump lf3 through a conduit l2 to the mixer which is indicated as a whole at 15. The mixer which is illustrateifl comprises in its construction a casing having a thus introduced overflows .trom one coin-- partnlent into the lcompartnir-.nt iininediatelv therehelow and is linally delivered through a valved discharge pipe l2 leading l'roin the lowest compartment.

The iti-oni the cooler are thoroughly mixed with the .solvent hv suitable i devices. lhese identical in 'torni and operation` and each comprises a hell-shaped casino* 253 ilroi'idcd with rui-hating hollow l for the einiseion olE lh-e gas into they hody oi the liquid. rl`he several florii-i-s'are allixed to a shall .27 which extends lhroupfh the top olE the casing. und is provided al iis.-

upper und with a pulleyv hy means ot which it may he drivcuhy poner-lrain-emitting mechanism lrpm aronvenicni power alnial'i. Allhe shall: projects ihrough the holoni oi the casingl into the pipe l! and is stepped in a hearing" therein. Through the partitions are openings to reci-ire the shalfl. (here heinp at ouch opening: short piece ol` pipe lll lo oon-A duct the gas inio the hollAshapcd casing therealmve. 'l`ho gas is thus` conducted in series` to the scvcrzl compartments und is dialrihuled through and mixed with lhc liquid. Huch gras. as is not ahsorhcd in the liquid in 'the lower compartment., passes therefrom inlo the roiuparlzueiu neil; allow and is mixed with iho liquid therein. .tiny unmixed las passes therefrom inlo ihil higher compartment aud is mixed will! the hodv olE solvent therein. 'the other gusci; escape thro-ugh a ronduit lefulingi4 l'rom the upper compartincnl.

'l`he solvent is l'orceii into the` compartment Q0 hy :i pump lil which is connected lo the inlet fl-"l hy pipes l'lfl. 'l. ll the initial temporal ure` ol' the solvent, on account of utmospherlc conditions, is in the vicinity olf 320 F., the solvent may pass directly lfrom thc pump lo the compartment lit, on the other hand, the initial temperature of the solvent is materially alcove 35.20 lf., it is lll() lll-ri temperature.

caused to pass through a refrigerating apparatus prior to its admission to .the mixer. At 36 a refrigerating apparatus is indicated which may be formed in any suitable man ner. As shown, it consists of a casing through Which the solvent passes and Whch contains a coil'of pipe through which a refrigerated brine or other refrigerant is circulated. In cold Weather, this cooler may be located out of doors and may be chilled or refrigerated by the normal out-of-door As shown, the solvent is conducted to the refrigerator by a pipe 3st and is conducted thence to the mixer by `a pipe 37. The coil for the refrigerant is indicated conventionally at 40. Suitable valves 38 and 39 may be provided to direct the solvent from the pump either to the mixer or through the refrigerator. The solvent is caused to' enter the mixer preferably at approximately 320 F. On account of the Sensible heat of the gases entering the solvent and on account of the heat liberated by the reactions taking place in the several compartments, the temperature of the mixture emitted from the lower compartment, unless the same is further refrigerated, Will be approximately 500 F. The temperature of the solvent, as it passes through the mixture, gradually rises and its absorption capacity gradually decreases.' Hence we may also provide means for retrigerating the mixture to compensate, to some extent at least, for the rise in temperature due to the chemical reactions vand to the sensible heat of the incoming gases, thereby insuring the production ot an acid liquor having a maximum predetermined proportion of free sulturous acid.

On the drawing it will be observed that We have located in the lower compartment 18 a refrigerating coil indicated at 41. Through this coil is passed any suitable refrigerant, suoli as an expanding` gas or a refrigerated brine. By this means, We are able to lower the temperature of the body of solvent materially to increase its absorption capacity and thus provide for the delivery of the solvent at a` predetermined temperature, say at a temperature of 45o F. or even lower, and containing a greater proportion of free sulturous acid than would otherwisebepossible. The solvent, which has been preliminarily refrigerated to a predetermined temperature, is circulated through the mixer, and the gas is introduced into the mixer so as to pass in a direction Y opposite to the llovv of the solvent. The un dissolved sulfur dioxid entering the upper chamber meetsthe coldest body of solvent, and is practically all absorbed thereby. The temperature ot the'solvent is raised, and it iiovvs into the next lower compartment Where its temperature is still further increased by the heat of the gases and the heat 'gas is initially delivered, and Where solvent.

of the reactions. Hence still more gas is absorbed, though the capacity of absorption is diminished. The solvent lovvs vfrom the second compartment toA the third or lowest compartment Where the incoming body ofl the sensible heat of the gas is greatest. .In this compartment, however, the solvent is refrigor-ated, and its vabsorption capacity, due toits rise in temperature, is more or less restored, with the result that the proportion of free sulfurous acid'contained in the et! fluent is increased. i i

lWe would not considerit a 4departure from the invention if each compartment in the mixer contained a coil for a refrigerant, so that each body of solvent could be refrigerated to compensate for its rise in temperature due to the heat imparted thereto by the gas.

lt is apparent that the present invention is not limited to the form of refrigerating apparatus illustrated, and that said apparatus may be varied according to prevailing conditions and Jfacilities as occasion requires to elect the desired refrigeration of tht So far as any generic featuresof the proc-! ess are concerned, this application is a continuation of our application Serial No. 9 541,244, tiled February 1, 1910.

What We claim is:

1. The-v herein described process o producing calcium bisultite having a predeten. mined proportion of free sulfurous acid, which consists in retrigerating'milk or lime to a constant predetermined temperature, and passing sulfur dioxid through saidvre' trigerated milk of' lime. l Y,

2. The herein described process of pro ducing calciumbisulte having a constant. predetermined proportion of :tree sulfurous acid, which consists in'preliminarily refrigerating milk of lime to approximately 32 F., and passing sulfur dioxid through said refrigerated milk of lime.

3. The herein described process which` consists in the following steps, to Wit: burning a sulfur-bearing substance, cooling the products of .combustion to condense those having a higher volatilizing point than sul fur dioxid, refrigerating milk of lime to a constant predetermined temperature, continuously supplying the retrigeratedmilk of lime to and mixing the sulfur dioxid With the refrigerated milk of lime in a suitable mixer, and continuously withdrawing from said mixer calcium bisulite-having a conlot stant predetermined proportion of free sulurous acid. f 105 mined temperature.

@img mined tempereture to eompeiiseee gioithe increase ini the heet of the eeiifeii due to' Mie mixing sulfur diexidi eheiewiih, und. ireiifg- @rating the mixture to e (sonstwie predeter- 5 The herein deecri process Gipfediieiiig calcium bisuim having a, ,constant predetermined propertiee' oi' free sulfureus acidj which 'consists im preiimineiily refrigereiting milk of ime Ee e predetermined `eeuperetuie7 passing seidv milk' of ime ehi-@ugh e mixer, passing sufur dioxid, inmhe oppoie miko iime iii the mixer, sind iefiigen lie' mixui'e te e constant piedetei'- ecimixure of ith-e ges 'with ehe, Seli/ene whereby 'she deeii'edeonsteni; prepoitien of :ieee eulfureus @eid-in the mixtui'e ie seeuiefis iure, and Withdfaiwiiig from said mixer milf; y

The herein described continuous proeeesV which consists in introducing milk of lime end sulfur diexid into e mixer, mixingthe seme therein, refiigei'eting the mixture in Aeeil mixer te e predetermined tempera?,

eium bisuiite having a consi-ent predeterff mined proportion of :f1-ee sulfurous acid. 111 eestimony whereof We have ,eiixed pun V`Signetiii'ee, in pi'esenee of two witnesses. site direeeioiimte and mixing the seme with 1 HUGH K. MUCRE.

Witnesses te Meme:

MARCUS B. MAY? V/'ieneseesfio VVH:

LILLIAN M. STUD, HERALD SHAW. 

